PAL SPME ArrowThe Better SPME

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PAL SPME ArrowThe new dimension for Solid-Phase Micro Extraction

SPME has become one of the most widely used extraction technologies for environmental, food and clinical analyses. It is well suited for automated sample preparation resulting in reduced time per sample, less sample manip-ulation and solvent consumption. However, the technology remained almost unchanged with some significant drawbacks, such as the limited mechanical stability and small phase volumes of the fibers.

The PAL SPME Arrow (patent pending) is a new technology for micro-ex-traction, combining trace level sensitivity with high mechanical robustness. The PAL SPME Arrow has an outer diameter of 1.1 or 1.5mm, resulting in large sorption phase surfaces and volumes. The arrow-shaped tip allows smooth penetration of vial and injector septa. In contrast to traditional SPME fibers, the Arrow design fully protects the sorptive material, minimizing ad-verse influences and loss of analytes during transfer processes. With the PAL RTC and RSI the SPME Arrow sampling is fully automated lead-ing to high productivity.

The figure below shows the dimension of a PAL SPME Arrow 1.5 mm (a),a PAL SPME Arrow 1.1 mm (b) and a SPME Fiber (c) in comparison.

a

b

c

PAL SPME Arrow:The new dimension of SPME

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HeadspaceExtractionTechniques

0.1 1 10 100 1000 Working range (ng/L)

ImmersionExtractionTechniques

Headspace (Syringe or Loop)

SPME Fiber

SPME Arrow

Purge & Trap

SPME

SPME Arrow

Better SPME

– Adaptation of existing SPME methods is straightforward – PAL SPME Arrow works well for headspace and immersion extraction – With the wide selection of sorption materials (cf. page 10) a wide variety of com-

pounds are now amenable to SPME – The PAL SPME Arrow is an ideal field sampling device

PAL SPME Arrow covers a wide range of applications. However, for dynamic headspace applications, especially for volatiles we recommend ITEX Dynamic Headspace (DHS). This powerful technology achieves ng/L sensitivities without the pitfalls of purge & trap systems.

What Better SPME means

= 2 x productivity

Bigger surface,faster extraction.

2 x higher sample throughput.

More sorption phase,superior sensitivity.

Up to 10 x more sensitivity - wider linear range.

Optimized geometry,greater robustness.

PAL SPME Arrows last at least 2 x longer. Injector septa last at least 2 x longer. Lower running costs.

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More Volume: Up to 10x more Sensitivity

The table below shows the dimension of a PAL SPME Arrow 1.5 mm (a), 1.1 mm (b) and a SPME Fiber (c) in comparison:

Sorption phase surface

Sorption phase volume

a 62.8 mm2 11.8 µL

b 44.0 mm2 3.8 µL

c 9.4 mm2 0.6 µL

Immersion Extraction: Polyaromatic Hydrocarbons (PAHs) in Water

0

10

20

30

40

50

60

70

Extraction yields for water samples containing PAHs @ 50 ng/L after 70 min. A PAL SPME Arrow 20 mm x 250 µm Carbon WR was compared to SPME fiber 10 mm x 100 µm Carbon WR immersion (Kremser et al., 2015).

Headspace Extraction: Aroma Analysis in White Wines

5 1 0 1 5 2 0 2 5 m in u te s

0 .0

2 .5

5 .0

7 .5

M C o u n ts

1

23 4

5

6

Chardonnay

1. Isoamylacetate2. Ethylhexanoat3. Ethyloctanoate4. Ethyldecanoate5. Phenylethylalcohol6. Octanoic acid

5 1 0 1 5 2 0 2 5 m in u te s

0 .0

2 .5

5 .0

7 .5

1 0 .0

M C o u n ts

1

Gewürztraminer

2

34

5

6

1. Isoamylacetate2. Ethylhexanoat3. Ethyloctanoate4. Ethyldecanoate5. Phenylethylalcohol6. Octanoic acid

Chromatograms showing the headspace extraction of aroma components from different white wines with PDMS fibers(PAL SPME Arrow 100 µm, 20 x 1.1 mm compared to SPME 100 µm, 10 x 0.3 mm)

Iodoform in Water

5 6 7 8 9 10 minutes

0

25

50

75

100

kCounts

Headspace

SPME Arrow26 x moresensitivity

5 6 7 8 9 10 minutes

0

10

20

30

37kCounts

Immersion

SPME Arrow6 x moresensitivity

Extraction of 1 µg/L iodoform from tap water with DVB fibers (headspace and immersion extraction), PAL SPME Arrow 100 µm, 20 x 1.1 mm compared to SPME 100 µm, 10 x 0.3 mm.

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Bigger Surface: 2x ThroughputImmersion Extraction: Polyaromatic Hydrocarbons (PAHs) in Water

0

10

20

30

40

50

60

70

80

90

Naphtalene Fluorene Benzo(a)pyrene

Relative immersion extraction yield (measured as % extracted after a 70 min) for PAHs at 50 ng/L with PDMS fibers(PAL SPME Arrow 100 µm, 20 x 1.1 mm compared to SPME 100 µm, 10 x 0.3 mm)

Headspace Extraction: Off Flavor Compounds in Water

0

200000

400000

600000

800000

1000000

1200000

DVB SPME Arrow DVB SPMERelative headspace extraction yield (measured as amount extracted after 30 min) for off-flavor compounds in water at 100 ng/L with DVB fibers. (PAL SPME Arrow 100 µm, 20 x 1.1 mm compared to SPME 100 µm, 10 x 0.3 mm)

References[1] Belardi R., Pawliszyn J., Water Pollut. Res.J.Can. 1989, 24, 179

[2] SPME Arrow - Evaluation of a Novel Solid-Phase Microextraction Device for Freely Dissolved PAHs in Water; Kremser A. et al., Anal. Bioanal. Chem. 2016, 408, 943-952

[3] Solid phase microextraction Arrow for the sampling of volatile amines in wastewater and atmosphere; Helin A. Et al., J. Chrom. A 2015, in press

[4] PAL System Application Notes: Determination of iodoform in drinking water by SPME and GC/MS and Determination of C2-C12 aldehydes by SPME on-fiber

derivatization and GCMS

With the PAL RTC and RSI the entire SPME process is fully automated. This guarantees process safety and high reproducibility.

PAL Heatex Stirrer - New Mixing and Heating Technologyfor Sample Preparation and SPME.

The powerful PAL Heatex Stirrer mixes samples rapidly applying cycloid shaped mixing patterns without the need for stir bars. For SPME headspace and immersion sampling the special design (pat. pending) ensures optimal performance.

The PAL Heatex Stirrer offers:– Rapid equilibration through effective stirring for headspace and immersion SPME sampling while ensuring the integrity of

the fiber– Efficient dissolution of solids, temperature controlled– Thorough liquid/liquid extraction– Stirring/heating for derivatization reactions– No stir bar required, constant stirring also with samples containing solids– No cross contamination– Precise control of the equilibration temperature 40-150 °C– Software controlled, temperature and stirring speed are logged

SPME Arrow Conditioning Extraction Desorption / Injection

SPME Arrow Tool

Agitator

SPME ArrowConditioning Module

Heatex Stirrer

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Ordering information for required parts

SPME Arrow Starter Kit(injector specific)

PNo.: see below

Starter Kit containing – SPME Arrow Tool – SPME Arrow Holder– SPME Arrow Selection of five different SPME Arrows– SPME Arrow Instruction Leaflet– Adapter Kit for GC injector (details see below)

Heatex Stirrer Module

PNo.: PAL3-HeatexStirrer

For mixing and heating in sample prep and SPME– Temperature range ambient temperature - 150 °C– Mixing speed up to 1600 rpm (200 cycloidal loops)– Optimized for 20 mL vials (for 10 mL vials a special adapter is required)

Agitator Module

PNo.: PAL3-Agitator

The Agitator Module provides 6 positions for 20 mL vials for incubation and agitation of samples.– Temperature range ambient temperature – 200 °C– Agitation speed 250 – 750 rpm– Optional adapters for 2 mL or 10 mL vials

Ordering information for optional modules

SPME Arrow Conditioning Module

PNo.: PAL3-SPME-ArrowCond

For the conditioning of SPME Arrow as well as SPME fibersprior to sample enrichment– Position for automated conditioning– Position for manual pre-conditioning– Automated purge gas valve– Manual gas valve for pre-conditioning– Replacement liners for easy maintenance

Ordering information for starter kits and suitable liners

Starter Kits PAL3-ARR-Start-GC2010 Starter Kit SPME Arrow for Shimadzu GC-2010 Plus consisting of: 1 Adaption Kit for the split/splitless injector of Shimadzu GC-2010 Plus (ARR-SSL-Inj-GC2010), 1 Liner Nut, 1 Screw Cap, 2 SPME Arrow Liner,1 SPME Arrow Tool Kit (PAL3-SPME-Arrow-Kit)

PAL3-ARR-Start-GC6890 Starter Kit SPME Arrow for Agilent GC6890 consisting of: 1 Adaption Kit for the split/splitless injector of Agilent GC 6890 (ARR-SSL-Inj-GC6890), 2 SPME Arrow Liners for SSL Injector of the Agilent GC 6890, 1 SPME Arrow Tool Kit (PAL3-SPME-Arrow-Kit)

PAL3-ARR-Start-GC7890 Starter Kit SPME Arrow for Agilent GC 7890 consisting of: 1 Adaption Kit for the split/splitless injector of Agilent GC 7890 (ARR-SSL-Inj-GC7890), 2 SPME Arrow Liners for SSL Injector of the Agilent GC 7890, 1 SPME Arrow Tool Kit (PAL3-SPME-Arrow-Kit)

PAL3-ARR-Start-Tr1300 Starter Kit SPME Arrow for Thermo GC Trace 1300/1310 consisting of: 1 Adaptation Kit for the split/splitless injector of Thermo GC Trace1300/1310 (ARR-SSL-Inj-Trace1300), 2 SPME Arrow Lin-ers for SSL Injector of Thermo GC Trace1300/1310, 1 SPME Arrow Tool Kit (PAL3-SPME-Arrow-Kit)

PAL3-ARR-Start-TrUltra Starter Kit SPME Arrow for Thermo GC Trace Ultra consisting of: 1 Adaptation Kit for the split/splitless injector of Thermo GC TraceUltra (ARR-SSL-Inj-TraceUltra), 2 SPME Arrow Liners for SSL Injector of Thermo GC TraceUltra, 1 SPME Arrow Tool Kit (PAL3-SPME-Arrow-Kit)

Suitable Liners ARR-Liner-CondModule Liner for SPME Arrow Conditioning Module, package containing 3 pcs

ARR-Liner-GC2010 SPME Arrow Liner for SSL Injector of SHIMADZU GC-2010 Plus, package containing 3 pcs

ARR-Liner-GC6890 SPME Arrow Liner for SSL Injector of AGILENT GC 6890, package containing 3 pcs

ARR-Liner-GC7890 SPME Arrow Liner for SSL Injector of AGILENT GC 7890, package containing 3 pcs

ARR-Liner-Trace1300 SPME Arrow Liner for SSL Injector of Thermo GC Trace1300, package containing 3 pcs

ARR-Liner-TraceUltra SPME Arrow Liner for SSL Injector of Thermo GC TraceUltra, package containing 3 pcs

PAL SPME Arrow Ordering InformationSystem requirements

– PAL RTC or RSI with firmware 2.3 or higher – PAL SPME Arrow Tool – PAL Agitator & Heatex Stirrer Module – Adaptation of GC-injector (see page 11) – A PAL SPME Arrow Conditioning Module is highly recommended, the PAL SPME Fiber Conditioning Module cannot be used with SPME Arrow.

The PAL SPME Arrows are available in order quantities of one, three or five SPME Arrows per box.For method development, a set of each fiber type (set of five) is available.

Diameter Phase Thickness Color Code Set of 1 SPME ArrowDescription PNo.

Set of 3 SPME ArrowsDescription PNo.

Set of 5 SPME ArrowsDescription PNo.

PDMS SPME Arrow (Polydimethylsiloxane)

1.1 mm 100 µm Red ARR11-P-100/20-P1 ARR11-P-100/20-P3 ARR11-P-100/20-P5

Acrylate SPME Arrow (Polyacrylate)

1.1 mm 100 µm Grey ARR11-A-100/20-P1 ARR11-A-100/20-P3 ARR11-A-100/20-P5

Carbon WR SPME Arrow / PDMS (Carbon Wide Range / PDMS)

1.1 mm 120 µm Light Blue ARR11-C-WR-120/20-P1 ARR11-C-WR-120/20-P3 ARR11-C-WR-120/20-P5

DVB SPME Arrow / PDMS (Divinylbenzene / PDMS)

1.1 mm 120 µm Violet ARR11-DVB-120/20-P1 ARR11-DVB-120/20-P3 ARR11-DVB-120/20-P5

PDMS SPME Arrow (Polydimethylsiloxane)

1.5 mm 250 µm Black ARR15-P-250/20-P1 ARR15-P-250/20-P3 ARR15-P-250/20-P5

SPME Arrow Collection – Development Kit

One of each type of SPME Arrows above | set of five ARR1115-SEL5-S1

(Detailed user information can be found in the SPME Arrow Instruction Leaflet.)

For more information on the PAL System visit:

www.palsystem.com

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PAL is a registered trademark of CTC Analytics AG, Switzerland